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Liquid chromatography-tandem mass spectrometry method for the estimation of adefovir in human plasma：Application to a pharmacokinetic study

Dipanjan GOSWAMI ; Sanjay GURULE ; Arabinda SAHA ; Poonam VATS ; Arshad KHUROO ; Tausif MONIF

Journal of Pharmaceutical Analysis.2015;(3):190-199.

An analytical method based on solid phase extraction was developed and validated for analysis of adefovir in human plasma. Adefovir-d4 was used as an internal standard and Synergi MAX RP80A (150 mm × 4.6 mm, 4μm) column provided the desired chromatographic separation of compounds followed by detection with mass spectrometry. The method used simple isocratic chromato-graphic condition and mass spectrometric detection in the positive ionization mode. The calibration curves were linear over the range of 0.50–42.47 ng/mL with the lower limit of quantitation validated at 0.50 ng/mL. Matrix effect was assessed by post-column infusion experiment to monitor phospholipids and post-extraction addition experiment was performed. The degree of matrix effect for adefovir was determined as 7.5%and ion-enhancement in five different lots of human plasma was 7.1%and had no impact on study samples analysis with 4.5 min run time. The intra- and inter-day precision values were within 7.7% and 7.8%, respectively, for adefovir at the lower limit of quantification level. Validated bioanalytical method was successfully applied to clinical sample analysis.

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Determination of diclofenac in pharmaceutical preparations by voltammetry and gas chromatography methods

Bilal YILMAZ ; Ulvihan CILTAS

Journal of Pharmaceutical Analysis.2015;(3):153-160.

Rapid, sensitive and specific methods were developed for the determination of diclofenac in pharmaceutical preparations by linear sweep voltammetry (LSV) and gas chromatography (GC) with mass spectrometry (MS) detection. The linearity was established over the concentration range of 5–35μg/mL for LSV and 0.25–5μg/mL for GC–MS method. The intra- and inter-day relative standard deviation (RSD) was less than 4.39% and 4.62% for LSV and GC–MS, respectively. Limits of quantification (LOQ) were determined as 4.8 and 0.15μg/mL for LSV and GC–MS, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial diclofenac dosage forms to quantify the drug and to check the formulation content uniformity.

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Isolation and characterization of a degradation product in leflunomide and a validated selective stability-indicating HPLC-UV method for their quantification

Balraj SAINI ; Gulshan BANSAL

Journal of Pharmaceutical Analysis.2015;(3):207-212.

Leflunomide (LLM) is subjected to forced degradation under conditions of hydrolysis, oxidation, dry heat, and photolysis as recommended by International Conference on Harmonization guideline Q1A(R2). In total, four degradation products (I–IV) were formed under different conditions. Products I, II and IV were formed in alkaline hydrolytic, acidic hydrolytic and alkaline photolytic conditions. LLM and all degradation products were optimally resolved by gradient elution over a C18 column. The major degradation product (IV) formed in hydrolytic alkaline conditions was isolated through column chromatography. Based on its 1H NMR, IR and mass spectral data, it was characterized as a British Pharmacopoeial impurity B. The HPLC method was found to be linear, accurate, precise, sensitive, specific, rugged and robust for quantification of LLM as well as product IV. Finally, the method was applied to stability testing of the commercially available LLM tablets.

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Selective extraction of dimethoate from cucumber samples by use of molecularly imprinted microspheres

Jiaojiao DU ; Ruixia GAO ; Hu YU ; Xiaojing LI ; Hui MU

Journal of Pharmaceutical Analysis.2015;(3):200-206.

Molecularly imprinted polymers for dimethoate recognition were synthesized by the precipitation polymerization technique using methyl methacrylate (MMA) as the functional monomer and ethylene glycol dimethacrylate (EGDMA) as the cross-linker. The morphology, adsorption and recognition properties were investigated by scanning electron microscopy (SEM), static adsorption test, and competitive adsorption test. To obtain the best selectivity and binding performance, the synthesis and adsorption conditions of MIPs were optimized through single factor experiments. Under the optimized conditions, the resultant polymers exhibited uniform size, satisfactory binding capacity and significant selectivity. Furthermore, the imprinted polymers were successfully applied as a specific solid-phase extractants combined with high performance liquid chromatography (HPLC) for determination of dimethoate residues in the cucumber samples. The average recoveries of three spiked samples ranged from 78.5% to 87.9% with the relative standard deviations (RSDs) less than 4.4% and the limit of detection (LOD) obtained for dimethoate as low as 2.3μg/mL.

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Determination of drug, excipients and coating distribution in pharmaceutical tablets using NIR-CI

Anna PALOU ; Jordi CRUZ ; Marcelo BLANCO ; Jaume TOMàIS ; Manel ALCALà

Journal of Pharmaceutical Analysis.2012;02(2):90-97. doi:10.1016/j.jpha.2011.11.003

The growing interest of the pharmaceutical industry in Near Infrared-Chemical Imaging (NIR-CI) is a result of its high usefulness for quality control analyses of drugs throughout their production process (particularly of its non-destructive nature and expeditious data acquisition).In this work,the concentration and distribution of the major and minor components of pharmaceutical tablets are determined and the spatial distribution from the internal and external sides has been obtained.In addition,the same NIR-CI allowed the coating thickness and its surface distribution to be quantified.Images were processed to extract the target data and calibration models constructed using the Partial Least Squares (PLS) algorithms.The concentrations of Active Pharmaceutical Ingredient (API) and excipients obtained for uncoated cores were essentially identical to the nominal values of the pharmaceutical formulation.But the predictive ability of the calibration models applied to the coated tablets decreased as the coating thickness increased.

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Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form

Deepak BAGESHWAR ; Vineeta KHANVILKAR ; Vilasrao KADAM

Journal of Pharmaceutical Analysis.2011;01(4):275-283. doi:10.1016/j.jpha.2011.09.012

A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v). This system was found to give compact and dense spots for both itopride hydrochloride (Rf value of 0.55±0.02) and pantoprazole sodium (Rf value of 0.85 ± 0.04). Densitometric analysis of both drugs was carried out in the reflectance-absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9988± 0.0012 in the concentration range of 100-400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9990±0.0008 in the concentration range of 200-1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method.

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An ionic liquid supported CeO2 nanoparticles-carbon nanotubes composite-enhanced electrochemical DNA-based sensor for the detection of Pb2+

Yan LI ; Xiaorong LIU ; Xiaohui NING ; Cancan HUANG ; Jianbin ZHENG ; Juncai ZHANG

Journal of Pharmaceutical Analysis.2011;01(4):258-263. doi:10.1016/j.jpha.2011.09.001

An electrochemical sensor incorporating a signal enhancement for the determination of lead (Ⅱ) ions (Pb2+) was designed on the basis of the thrombin-binding aptamer (TBA) as a molecular recognition element and ionic liquid supported cerium oxide (CeO2) nanoparticles-carbon nanotubes composite modification. The composite comprises nanoparticles CeO2, multi-wall carbon nanotubes (MWNTs)and hydrophobic room temperature ionic liquid (RTIL) l-ethyl-3-methylimidazolium tetrafluoroborate (EM1MBF4). The electrochemical sensors were fabricated by immersing the CeO2-MWNTs-EMIMBF4 modified glassy carbon electrode (GCE) into the solution of TBA probe. In the presence of Pb2+, the TBA probe could form stable G-quartet structure by the specific binding interactions between Pb2+ and TBA. The TBA-bound Pb2+ can be electrochemically reduced, which provides a readout signal for quantitative detection of Pb2+. The reduction peak current is linearly related to the concentration of Pb2+ from 1.0 × 10 8 M to 1.0 × 10-5 M with a detection limit of 5 × 109 M. This work demonstrates that the CeO2-MWNTs-EMIMBF4 nanocomposite modified GCE provides a promising platform for immobilizing the TBA probe and enhancing the sensitivity of the DNA-based sensors.

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Glassy carbon electrode modified with multi-walled carbon nanotubes sensor for the quantification of antihistamine drug pheniramine in solubilized systems

Rajeev JAIN ; Sanjay SHARMA

Journal of Pharmaceutical Analysis.2012;02(1):56-61. doi:10.1016/j.jpha.2011.09.013

A sensitive electroanalytical method for quantification of pheniramine in pharmaceutical formulation has been investigated on the basis of the enhanced electrochemical response at glassy carbon electrode modified with multi-walled carbon nanotubes in the presence of sodium lauryl sulfate.The experimental results suggest that the phcniramine in anionic surfactant solution exhibits electrocatalytic effect resulting in a marked enhancement of the peak current response.Peak current response is linearly dependent on the concentration of pheniramine in the range 200-1500 μg/mL with correlation coefficient 0.9987.The limit of detection is 58.31 μg/m L.The modified electrode shows good sensitivity and repeatability.

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Determination of fluoroquinolones, sulfonamides,and tetracyclines multiresidues simultaneously in porcine tissue by MSPD and HPLC-DAD

Hu YU ; Hui MU ; Yingmei HU

Journal of Pharmaceutical Analysis.2012;02(1):76-81. doi:10.1016/j.jpha.2011.09.007

An efficient method is provided to detect simultaneously some important veterinary drugs from different classes in highly complex animal tissue matrix.This method using matrix solid-phase dispersion (MSPD) and high performance liquid chromatography (HPLC) with diode array detection (DAD) is developed to effectively determine two fluoroquinolones (enoxacin and lomefloxacin),two sulfonamides (sulfanilamide and sulfamethoxazole) and one tetracycline (tetracycline) simultaneously in porcine tissues.In the process,MSPD methodology was used to treat samples,washed by n-hexane to remove lipid,eluted the analytes with acetonitrile-dichloromethane (1∶1,v/v).Solvent acetonitrile and solvent acetic acid (0.1％) were combined in a gradient.HPLC-DAD analysis of the tissue samples was performed within 15min at a flow rate of 1.0mL/min.The results showed that a recovery at 0.1,0.5 and 1.0 μg/g fortification levels ranged from 80.6％ to 99.2％ with satisfactory relative standard deviations (RSDs) (below 6.1％.n=3) and the limits of quantitation (LOQ) ranged from 7 μg/kg to 34 μg/kg in porcine tissues.Utilization of the method in successfully simultaneous analysis of porcine tissue incurred with veterinary drug multiresidues is described.

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A validated stability-indicating LC method for the separation of enantiomer and potential impurities of Linezolid using polar organic mode

T.satyanarayana RAJU ; O.vishweshwari KUTTY ; P.yadagiri SWAMY

Journal of Pharmaceutical Analysis.2012;02(4):272-278.

Although a number of methods are available for evaluating Linezolid and its possible impurities,a common method for separation if its potential impurities,degradants and enantiomer in a single method with good efficiency remain unavailable.With the objective of developing an advanced method with shorter runtimes,a simple,precise,accurate stability-indicating LC method was developed for the determination of purity of Linezolid drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products.This method is capable of separating all the related substances of Linezolid along with the chiral impurity.This method can also be used for the estimation of assay of Linezolid in drug substance as well as in drug product.The method was developed using Chiralpak IA (250 mm × 4.6 mm,5 μm) column.A mixture of acetonitrile,ethanol,n-butyl amine and trifluoro acetic acid in 96:4:0.10:0.16 (v/v/v/v) ratio was used as a mobile phase.The eluted compounds were monitored at 254 nm.Linezolid was subjected to the stress conditions of oxidative,acid,base,hydrolytic,thermal and photolytic degradation.The degradation products were well resolved from main peak and its impurities,proving the stability-indicating power of the method.The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity,limit of detection,limit of quantification,precision,linearity,accuracy,robustness and system suitability.

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